Process of and apparatus for distilling petroleum.



J. W. VAN DYKE & W. M. IRISH. PROCESS OF AND APPARATUS FOR DISTILLING PETROLEUM.

APPLICATION FILED APR.1B, 1911.

Patented May 5, 1914.

, fnz/eizzars 4AM xzmhgk JOHN W. VAN DYKE AND WILLIAIM M. IRISH, OF PHILADELPHIA, PENNSYLVANIA,

ASSIGNORS TO THE ATLANTIC REFINING COMPANY, OF PHILADELPHIA, PENN SYLVANIA, A CORPORATION OF PENNSYLVANIA. I 1

Process OF AND APPARATUS FOR DISTILLING PETROLEUM.

Specification of Letters Patent.

Patented May 5, rare.

Application filed April 18, 1911. Serial No. 621,905.

of an undistilled residue for obtaining therefrom a wide range of products in the same run; the distillation being performed at least in part at the high temperatures necessary to evaporate hydrocarbons with boiling points above 600 'F. or above the temperature of commencement of cracking when this is below 600 F.; but the invention extends also to such distillation of petroleum in the form of a distillate and-to other distillations of distillateand of undistilled petroleum.

Each of the improvements composing the invention is intended to be secured for all the uses to which it can be applied, with or without modification.

The object of the invention is mainly to enable the early runnings of distillate in distilling a charge of oil .to be obtained in a purer state than that in which they would be apt otherwise to be.

At the end of each run, before opening the still for cleaning it out in preparation for a new run, it has been the practice (which we retain) to fill the still with free steam, in order to expel therefrom the hydrocarbon vapors which then occupy the still. In prior current practice these vapors with the steam have been passed through the regular vapor passage; and, being carried by the steam into all parts of the condensers, they have condensed on the walls thereof and have remained (as we have discovered) in part at least attached thereto until dissolved off by the distillate which constitutes the earlier runnings of the next run. Their presence in said earlier runnings of distillate is particularly objectionable where a wide range of products is obtained in the same run (as in a continuous complete distillation of crude petroleum) because the vaporized hydrocarbons in the still at the end of a run in such case are, in gravity, color and properties, so far removed from those which compose the earlier runnings of the next run, that even a small proportion of the former manifests itself in the latter'and may make it necessary to redistill an otherwise satisfactory distillate. In any case, there would necessarily be a certain deterioration of said earlier runnings.

In accordance with the present invention, the vapors in the still at the end of each run are not allowed to pass on to the regular condenser-s, but are discharged mingled with the steam through a side passage adapted to that purpose, the same being arranged with special reference to the disposal of a comparatively small quantity of heavy vapors mixed with steam and best leading to a special condenser and receiver; so that the first distillate of the nextrun is received from the regular condenser free from any of the hydrocarbons composing the so expelled vapors. If desired, also,-more or less vapors before the termination of the run can be passed over through the same side passage. Where there is a series of condensers any one or more of these can be protected by withdrawal of vapors through such side passage before they reach the condenser or condensers. It is less important to keep contaminating vapors from condensers from which condensate is to be returned to the oil 1 in distillation than those from which distillate is to be received; but it is considered best to protect each condenser; since this can be done without more difficulty. The distillation which precedes the expulsion of the vapors as herein claimed is primarily. de: signed to be performed under atmospheric pressure and Without introduction of steam or other aeriform fluid into the still; but working under other pressures (as under partial vacuum, for example) and with injection of steam or other aeriform fluid into the still, or with either of these features separately, may to-some extent at least be employed, if so desired.

The invention comprisesall and singular the new, useful and original parts, improve ments and combinations herein claimed, whether of process or of apparatus. The accompanying drawing is a view partly in perspective and partly in vertical (longitudinal and cross) sections of a distilling apparatus in accordance with the present in vention,

, against loss of heat externally. There is a pipe 9 for filling the still with oil and a pipe h for conducting away the vapors to the regular condensing means. This vapor pipe h is connected with the vapor space of the still a by means of a short upright pipe 2' havinga removable cover 70. A. side opening receives the end of the vapor pipe h. Below said side opening is a flap valve whose opshould it tend to exceed the predetermined crating handle is seen at Z; and below said valve is another side opening which receives the pipe m, a continuation of which is formed by pipe or having a valve 7). In running the flap valve is open andthe valve closed. At the end of a run, when steam is introduced into the still to expel the vapors therefrom, their positions are reversed. 1 The pipe 9, which joins the pipe m, is provided with a safety valve r and a vacuum valve 8. A pipe t is provided for introducing steam into the'still at the end of a run before opening the manholes (one of which is shown at u) for cleaning out. As shown the vapor pipe it leads to a condenser in the form of numerous pipes 2 arranged in parallel between header 3 and chamber 4;. A light valve 6 in which a strictured outlet 5 is formed for the vapors may advantageously rest by its own weight over the end of each of a number of such pipes; so

that the lifting'of one or more of said valves may relieve the pressure in said pipes 2,

limit. There may be such a valve for'each of said pipes; but the pressure could, of course, be relieved without having so many valves. The pipes 2 are inclosed in a casing 7 which fits around the header 3 at the top and has inlet openings 8 at the bottom for inflow of air from'the surrounding atmosphere. Each inlet is provided with a valve 9, whichcan be opened, wholly or in part, or can be completely closed, as may be den sired. Air currents are produced in the casing 7 by heat absorbed from the walls of pipes 2. The chamber 4 is provided with a non-conducting (or heat retaining) jacket 10. In the chamber 4, resting on the grate 11, are pieces 12 of solid material, say cobble stones of four to eight inches in diameter. The vapor pipe 72. leads from the still directly to the space in chamber 4 below said grate 11. The vapor outlet of the condenser 2, 3, 4 is connected by pipes 13 with the vapor inlet of a second partial condenser 14 composed of numerous pipes set between headers and exposed to the air for cooling.

While dimensions and proportions can be varied, good results have been attained for a still holding a thousand'barrels of oil up tothe usual level with an aircooledcondenser having fifty six of the pipes 2, each eleven feet in length and four inches in exi ternal diameter (giving about 6 65 square feet ofcooling surface on the closely apt preached heat conducting wallsof pipes 2). A circular vapor'outlet opening5 of an inch each pipe 2, the vapor pipe it having an internal diameter of twelve inches and the valies 6 weighing about thirty three ounces eac The vapor outlet from condenser 14 is connected by pipe 15 with a water cooled. con denser, shown in the form of a coil 16 placed in a water tank 17, which is supported on walls 18 and cross beams 19. Thus, as shown, the vapors from the still a flow successively through two partial condensers each of them cooled by aeriform fluid, and then through a water cooled condenser.

The liquid outlets 20 and 21 of the pan tial condensers are respectively connected through U traps with the valved draw off pipes 22 and 23 placed in water tank 17. A valved draw off pipe 24 and a run back 25 (leading to the still a) are also connected with the liquid outlet 20. At 26 is a cover to exclude rain, in case the still stands out of doors. A valved pipe 27, shown in. dotted lines, can be used as a run back, if desired, between the condenser 14 and the still a.

The present invention is primarily designed for (but is not restricted to) a com plete distillation of crude petroleum in a continuous run, which is one of the modes set forth in our application of October 4,

sion and continuatlon, the division being made solely in consequence of olficial re quirement. In carrying out such complete the respective inventions hereof and of our said application 520,937, it is advantageous .to employ proceduresand appliances of condensation which are arranged for separating from each other hydrocarbons that are vaporized together; and it is most advantageous so to employ those procedures and appliances of condensation which are disclosed herein and in our said application 520,937 and in our application of April 18,

claims of this last mentioned application. This'last is likewise a division and continuation of our application 520,937, the divioflicial requirement. Other known or suit tion (as well as those last above mentioned) can be used in carrying out the respective inventions hereof and of our said application 520,937.

The expulsion of the vapors from the atthe end of a run and the appliances for accomplishing such expulsion, as recited in and a quarter diameter would suffice for 1909, No. 520,937; of which application the, application for the present patent is a divi distillation, as also generally in carrying out 1911, No. 621,904: and are recited-in the.

sion being made solely in consequence ofable procedures and appliances of condensastill the claims hereof, are no part of the invention of our application 520,937 as restricted ing temperatures; and the heating is con- I B. or heavier at 60. F.

tinued with gradual rise of temperature until the still contents become dry or nearly so,

wax tailings (of a gravity equivalent to 10 coming over as the last distillate. While the oil in the still is attaining a temperature of say 600 F. the temperature in header 3 may well rise to above 400 F. (480 F. was observed in a test run) and as the oil in distillation rises above 600 F. (say finally to 850 E, which has been observed) the temperature in the header 3 would bestbe between 400 F. and 600 F. (temperatures of from 470 F. to 607 were observed in said test run) al-- though near the end of the run the flow of vapors may become so small that the temperature in said header 3 would fall below 400 F. (317 F. was observed in said test run).

The cdndensate formed in the condenser 2, 3, 4 is returned to the still a during the earlier part of the run, say until the oil in distillation attains a temperature of about 700 F. (the run back .25 being then open. and the draw ofis 22 and 24 closed). Afterward the run back 25 is closed; and thecon- 'densate from condenser 2,3,4 is collected as distillate through the draw ofi's 22 and 24, running through the former while it remains sufliciently fiuid to do so.

The air inlet valves 9 would be more nearly closed at the beginning of each run,

when light hydrocarbons are'beingdistilled,

and'also at the end of each run when the vol ume ofvapors is-comparatively small, than they would be during the intermediate part of the run. In other words, the currents of cooling fluid are controlled to increase and decreasein a general way the cooling effect on .the vapors according to the varyingvollime and temperature of the "latter. Said air inlet valves 9 would also be closed more when the weather'is coldor windy and less (if at all) when it is warm or still. The valves 9 can also be manipulated to counteract or to compensate for other variables. In general observation of the streams from the respective condenser outlets, with test of samples if thought .expedient, should give sufiicient indications.

I Inthe test run, after bringing in the still, 147 barrels of dis- 211 barrels fromcondenser 14 during the time (19 hours and '20 minutes) in which the.

rels from condenser 2, 3, 4 during the time (17 'hours) in which the run was completed after the oil in distillation had attained about 700 F., anaverage collection from the first two condensers of 11 barrels per hour and from all three condensers of 27% barrels per hour.

At the end of the run the valve p in pipe n i is opened and the valve l 'is turned to close the ordinary vapor pipe 71-. Steam is then introduced through the pipe 6. ltfills the still a and expels the hydrocarbon vapors. They pass, with steam. through the pipes m n to any desired place or receptacle without entering the condenser 2, 3, 4, the condenser 14, or the condenser 16; so that at the nextrun the first runnings of condensate are not composed in part of hydrocarbons expelled by the steam. So far as concerns the con-' densate from condenser 2, 3', 4, as this re: ttu'ns to still a, the presence in it of said hydrocarbons would be of small importance,

and it is, therefore, of'minor importance for the valve Z and valved branch pipe n to be between condenser 2, 3, 4 and the still an, After expulsion of hydrocarbon vapors, the

steam is shut off; and thestill a is allowed to cool, is opened, is cleaned, is closed and then receives a new charge of petroleum.

Were the side passage n to remain closed and the regular vapor pipe? to remain open during the expulsion by steam of the vapors from the still (1 the Heavy hydrocarbons would (according to our experience) be carried in part even into the water cooled condenser 16 and would. remain adherent to the surfaces of said condenser 16. as well as of the condensers 14 and 2, 3, 4. I At the beginning'of the next run. the'heavy hydrocan bons in condenser 2. '3, 4 would be washed back into the still by the returning 'condensate; but-the distillate received from theremaining condensers would be deteriorated-by the heavy hydrocarbons which theywould dissolve from the condenser surfaces v By using ,the'run back 27 and opening it at the beginning of the next, the heavyhydroc'arbons could be washed back into thestill; but herein above referred to,

there would then be 'a loss ofltime (and conj sequently anexpense) which it is desirable -tillate were. received from condenser '16 and to avoid; and the distillate from condenser 16would still be contaminated by the heavyhydrocarbons which the steam Wouldcarry overinto it.

v We claim herein as our invention or discovery: p

1. The improvement in distilling petroleum, consisting in closing communication at the end of a run between the still and a distillate condenser, opening "at such time also a passage leading elsewhere and not to said condenser, and introducing free steam into the still to expel the vapors then remaining therein without introducing themducing free steam into the still to expel the vapors then remaining therein without in troducing them intosaid condensing means, charging the still with petroleum for a new run, conducting vapors again to said means, condensing.them therein as distillate, and so continuing, substantially as described.

v3. The improvement in distilling petroleum, consisting in charging a still withoil whose hydrocarbons have a wide range of boiling points, heating the same with gradual rise of temperature until vapors to give a wide range "of products have passed over, condensing such vapors largely at least in the same condensing means, closing communication at" the end of the run between the still and a distillate condenser,

opening at such time also a passage leading elsewhere and notto said condenser, and introducing free steam into the still to expel the vapors then remaining therein without introducing them into said condenser, s0

' that the early runnings of distillate which flow from said condenser in the next run shall be free from hydrocarbons composing the so expelled vapors, substantially as described. j

4. Apparatus for distilling petroleum, consisting of a still, a valved steam pipe opening into said still, a condenser for distillate, a vapor pipe leading from said still to said condenser, a passage leading away from said still without leading to said con-v denser and arranged with special reference to the disposal of vapors expelled from the still at the end of each run, and means whereby the vapor contents of said stiltcan at will either be directed into said condenser or be discharged elsewhere while shut oii from the latter, substantially as described.

Apparatus for distilling petroleum,

noeneas consisting of a still, a valved steam pipe opening -into said still, a condenser for distillate, a vapor pipe leading from said still to said condenser, a passage branching from said vapor pipe and leading away from it without leading to said condenser and aranged with special reference to the disposal of vapors: expelled from the still at the end of each run, and means arranged in one positionof the same to close said passage and open communicationbet-ween the portions of said vapor pipe on the still side and the condenserside respectively of said means and in another position to open said passage and close such communication, substantially as described.

6. The improvement in distilling petr0- which condensate of irel'atively lighter gravity is formed, opening at such time a passage leading elsewhere and not to the last mentioned condenser, and while said communication is closed and said passage open introducing free steam into the still'to expel the vapors then remaining therein without introducing them into the last mentioned condenser, substantially as described.

7. Apparatus for distilling petroleum,

consisting of a still arranged for its contents to be heated condnctivel'y, a valved steam pipe opening into said still, a number of condensers connected with each other in series and arranged to be maintained at difi'erent temperatures and one of them connected with the vapor space of saidstill so as to form condensates of different gravities corresponding with the respective condensers of the series, means for withdrawing said condensates separately from each other, means for closing communication when required between said still and a condenser in which condensate ofrelativelyglighter gravity is formed, a passage leading from the vapor space of said still elsewhcreand not to the last mentioned condenser and arranged with special reference to the disposal of vapors expelled from the still at the end of each run. and means for opening said passage when required, so that the vapors in said still can be expelled by steam without introducing them into the last mentioned condenser,

substantially as described.

milk

mews g '8. The improvement in'distilling petroleum, consistingjin charging a still With oil 1 whose hydrocarbons have a wide range of boiling points,

heating said oil conductively in order to evaporate therefrom hydrocarbons with, a wide range of boiling points,

conducting the vapors ofsuch evaporation through a number of condensers connected said portion of the condensing means in which condensate of lighter gravity is formed, introducing free steam into said still while said communication is closed and said passage open in order to expel the vapors then remaining in said still through said passage without letting them into said portion of the condenser series, recharging said still with oil to be distilled, closing said pa's sage, opening said communication between said still and said series of condensers, heating said ,oil conductively in order to evapo- .d'ensers rately time condensate to the oil in distillation rate the same, conducting the vapors-of such evaporation through said series of conwithdrawing. the condensates sepai-rom each other, and returning for a from that portion' of the condenser series in which condensate of heavier gravity is formed, that portion of the condenser series in which condensate of lighter gravity is formed being thus protected against ingress of heavier hydrocarbons during each run by the previous condensation of the latter in the warmer portion of the condenser series and during the expulsion of the vapors by free steam at the close of each run by the discharge of the vapors at such time through 7 said passage, and that portion of the con-- denser series in which condensateof heavier gravity is formed bein Washed at the beginning of each run by t close of each --ru' n by:

and that that e condensate which lis are aeraeaeaaae 011 a distillation, substantially as described.

I arranged for its contents to be heated condu'ctively, a valved steam pipe opening into said still, anumberof condensers connected with: each otherin series and arranged to be maintained at difierent temperatures and one of them connected with the vapor space of said still soas to ,form condensates of' difierent gravities'eorf 9. Apparatusfor distilling petroleum, conc s'ist'ing of astill 5 5- 1 responding with the respective condensers of Y the series, meansfor' withdrawing said condensates separately from each other and for temporarily returning condensate to the oil in distillation from that portion of said condenser series in which condensate of heavier gravity is formed, means for closing communication when required between said still and that portion at least-of saidcondenser series in which condensate of lightergravity is formed, a passage leading from the vapor space of saidstill elsewhere and not to" said portion of the condenser series in. which condensate of lighter gravity is formed andarranged with special referenceto the dis posal of vapors expelled from the still at the s end of each run, and means for opening said passage when required,. so that that portion of the'condenser series in which condensate of lighter gravity is formed can be protected againstingress of heavier-hydro f-carbons during each run by theprevious' condensation of the latter in the warmer portion of the condenser series and duringv the expulsion of the vapors,v by free steam at the the dischargeof the time- ,through said passage, ortion of the condenser series in which condensate of heavier gravity is formed can be washed at the beginning of vapors at such each run by condensate that is temporarily returned to the oil .indistill'ation, substantially as described. v

In testimony whereof we afiix our signatures in presence of two witnesses.

' a-JOHN W. VAN DYKE. a WILLIAM M. IRISH. Witnesses: v V

W. D. Ammnson,

C. WAITE. 

